CN114002406A - Method, system, equipment and application for collecting organic carbon content data of solid sample - Google Patents
Method, system, equipment and application for collecting organic carbon content data of solid sample Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 53
- 239000007787 solid Substances 0.000 title claims abstract description 44
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- 239000001569 carbon dioxide Substances 0.000 description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
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- 238000001745 non-dispersive infrared spectroscopy Methods 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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Abstract
The invention belongs to the technical field of organic carbon content data processing in solid samples such as soil, sediment and the like, and discloses a method, a system, equipment and application for acquiring organic carbon content data of a solid sample, wherein an electric signal automatic acquisition termination function of an instrument is closed; retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value, and monitoring the slope change in real time; the curve returns to the baseline, and a dialog box is popped up when a preset slope threshold value is reached, namely whether the analysis is finished or not or the analysis is continued according to the detection setting time; the operator judges that the data acquisition is finished, and selects to finish the analysis, and then the next sample is detected; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested. According to the invention, each sample is saved by about 4 minutes, so that the working efficiency is improved; for the sample with complex matrix, the accuracy of the detection result and the precision of the repeated measurement of the sample are improved.
Description
Technical Field
The invention belongs to the technical field of organic carbon content data processing in solid samples such as soil, sediment and the like, and particularly relates to a method, a system, equipment and application for acquiring the organic carbon content data of the solid samples.
Background
At present, when the existing instrument (Shimadzu TOC-L + SSM5000) is used for analyzing a solid sample, the main working principle is as follows: injecting the weighed sample into a TC combustion tube filled with oxidation catalyst by using a high-temperature catalytic combustion method, heating to 900 ℃, decomposing the TC in the sample into carbon dioxide by combustion, introducing combustion products into a non-infrared gas analysis part (NDR) pool through carrier gas, and detecting the carbon dioxide. The detection peak area of NDIR was calculated in the data processing section. Since the peak area is proportional to the TC concentration in the sample, the TC concentration in the sample is measured by obtaining a relational expression between the TC concentration and the peak area using a TC standard substance in advance. Next, the sample was subjected to acidolysis treatment with phosphoric acid at 200 ℃ to convert carbonate into carbon dioxide, which was introduced into a detector via a carrier gas, and the concentration of IC was calculated as in the TC detection method. The difference between the total carbon and the inorganic carbon is the content of the total organic carbon.
The existing instrument (Shimadzu TOC-L + SSM5000) has the following defects:
in the actual operation process, when a sample chamber is opened and samples are added or replaced, air is introduced into the whole system, a sensitive NDIR detector can detect trace carbon dioxide in the air, so that fluctuation of a base line is caused, about 2min is required to wait after the samples are replaced each time, the carbon dioxide peak in the air is waited to be discharged, the actual sample test can be started after the base line is stable, if the carbon dioxide detection in the air is not waited to be finished, the actual samples are detected after the base line is stable, the actual sample detection is easily finished in advance, (the return-to-zero detection process of the default base line of the system is finished), and the sample detection fails.
Secondly, in the measuring process, the inorganic carbon reacts slowly with the phosphoric acid due to the matrix effect of the sample and the like, the peak time and the peak shape in the detection process are directly influenced, when the electric signal of the detector tends to be a baseline, the default detection process of the system is finished, and the data acquisition process is terminated.
And setting the acquisition time of the instrument to be similar to the nominal acquisition time.
Through the above analysis, the problems and defects of the prior art are as follows:
(1) the data acquisition of the existing instrument is in an automatic termination mode, namely the data acquisition is finished when the slope change of the detected electric signal is smaller than a fixed value in a specified time; when the sample is replaced, the air peak of about 2min needs to be waited, and the working efficiency is reduced.
(2) For a sample with slow reaction, data acquisition is finished in advance, the content of inorganic carbon in the actual sample cannot be objectively reflected by a measurement result, and finally the content of organic carbon is inaccurate to measure.
The difficulty in solving the above problems and defects is: how to close the data to automatically terminate the acquisition is changed into a manual mode and an automatic mixed mode.
The significance of solving the problems and the defects is as follows:
(1) the method realizes the direct measurement without waiting in the process of replacing the sample, and greatly improves the working efficiency.
(2) The integrity of sample data acquisition is realized, and the accuracy of the result is greatly improved.
(3) The selectivity of manual termination of data collection and automatic collection is realized, and the measurement requirements of different types of samples are met.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method, a system, equipment and application for collecting organic carbon content data of a solid sample.
The invention is realized in such a way that a solid sample organic carbon content data acquisition method comprises the following steps:
calculating the instant slope of the visual interface peak-shaped curve and monitoring the change of the slope;
closing the automatic acquisition termination function of the instrument, recording the data of curve change and monitoring the slope;
and judging whether to terminate data acquisition or continue data acquisition according to the curve regression baseline.
The invention closes the automatic acquisition termination function of the instrument, enables data to be acquired all the time, can detect carbon dioxide generated by subsequent reaction of a sample with a complex matrix, and ensures the working efficiency and the accuracy of the detection result.
Further, the method for acquiring the organic carbon content data of the solid sample comprises the following steps:
firstly, closing the automatic acquisition termination function of an electric signal of an instrument;
secondly, retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value, and monitoring the slope change in real time;
thirdly, the curve returns to the base line, and a dialog box is popped up when the preset slope threshold value is reached, namely whether the analysis is finished or not is judged or the analysis is continued according to the detection setting time;
fourthly, judging that the data acquisition is finished by an operator, selecting to finish the analysis, and detecting the next sample; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested.
In the invention, in the first step, the continuous data acquisition is ensured, and the accuracy of the measurement result of the carbon dioxide in the sample with slow reaction is ensured. In the second step, a dialog box signal in the third step is given for monitoring whether data acquisition is finished; and fourthly, making a selection according to the experience of an operator, and improving the efficiency.
Further, the method for acquiring the organic carbon content data of the solid sample sets a threshold value, and judges whether the bulge of the signal curve can become a peak or not; in the process, a signal curve has fluctuation, so that the slope change of the curve is brought, and if the slope of the curve is greater than the set slope sensitivity, the curve is the starting point of a peak; when the slope of the curve falls below the slope sensitivity, it is the end point of the peak, and the peak is located between the start point and the end point.
The method for judging whether the bulge of the signal curve can become a peak comprises the following steps:
the formula for calculating the starting point of the peak of the curve is:
div (i, j) represents an objective coefficient of the calculated current curve peak i and the set curve peak j, and time (i), time (j) respectively represents data time from the beginning to the change of the current curve peak i and the set curve peak j, a numerator is an absolute value of a time difference between the change of the current curve peak i and the change of the set curve peak j, and a denominator is a sum of the change of the time between the change of the current curve peak i and the change of the set curve peak j;
the end point formula for the peak of the curve is calculated as:
αdiv(i,j)+βyi+λyj；
wherein div (i, j) represents the end point correlation degree of the current curve peak i and the set curve peak of j, yiAnd yjRespectively representing the memory rates of curve peaks i and j; α, β, λ are the weight values of the features.
Further, the slope calculation equation of the data acquisition process curve of the solid sample organic carbon content data acquisition method is as follows: the measuring result signal forms a curve equation with f (X, Y) being 0, P (X, Y) being any point on the curve, calculating the slope of the point on the curve, and calculating the derivative of the function f (X, Y) being 0 at X being X;
determining a function y (y) (x) by equation f (x, y) being 0, substituting y (x) into the equation to obtain an identity f [ x, y (x) 0, and calculating the full derivative of the function;
Calculating the slope:
by using the calculation model, the curve slope can be conveniently and accurately calculated in real time, and the real-time monitoring of curve change is realized.
It is a further object of the present invention to provide a computer apparatus comprising a memory and a processor, the memory storing a computer program which, when executed by the processor, causes the processor to perform the steps of the method for collecting organic carbon content data of a solid sample.
It is another object of the present invention to provide a computer-readable storage medium storing a computer program which, when executed by a processor, causes the processor to perform the steps of the method for collecting organic carbon content data of a solid sample.
The invention also aims to provide an information data processing terminal which is used for realizing the steps of the method for acquiring the organic carbon content data of the solid sample.
Another object of the present invention is to provide a solid sample organic carbon content data collecting system for implementing the solid sample organic carbon content data collecting method, the solid sample organic carbon content data collecting system comprising:
the function closing module is used for closing the automatic acquisition termination function of the electric signal;
the slope change monitoring module is used for retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value and monitoring the slope change in real time;
the detection time setting module is used for returning the curve to the baseline, and popping up a dialog box when a preset slope threshold value is reached, namely whether the analysis is finished or not or the analysis is continued according to the detection setting time;
the data acquisition ending judging module is used for judging that the data acquisition is finished by an operator, selecting to end the analysis and detecting the next sample; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested.
The invention also aims to provide an application of the solid sample organic carbon content data acquisition method in the organic carbon content data processing of the soil sample.
The invention also aims to provide application of the method for acquiring the organic carbon content data of the solid sample in processing the organic carbon content data in the sediment sample.
By combining all the technical schemes, the invention has the advantages and positive effects that: according to the data acquisition method established by the invention, the carbon dioxide peak in the air does not need to be waited in the process of replacing different samples, each sample can be saved by about 4 minutes, and the working efficiency is greatly improved; for a sample with a complex matrix, the data acquisition is complete and objective, the accuracy of the detection result is greatly improved, and the precision of the repeated measurement of the sample is improved.
TABLE 1 comparison of data from sample measurements before and after the application of the invention
As can be seen from the test data in Table 1, the influence on the measurement results of TC before and after the present invention is small because the TC is measured at 900 ℃ and the combustion is sufficient; for IC, because the reaction between the sample matrix and phosphoric acid is slow, the data acquisition process is terminated early, the original IC data acquisition is incomplete, the final data is small, and the TOC value is large.
The results of the measurement on the sample C21042P in table 1 are examples of the sample measurement before and after the application of the present invention, and the comparison shows that the effect of improving the accuracy of the detection is significant.
After the method is utilized, the data acquisition is complete, the IC content can be objectively reflected, and the data accuracy is high. Taking the standard sample GSS-8 as an example, the reference TOC value is 0.30%, the original calculation result is 0.694%, and the current result is 0.303%, which is relatively accurate.
Drawings
FIG. 1 is a flow chart of a method for collecting organic carbon content data of a solid sample according to an embodiment of the present invention.
FIG. 2 is a schematic structural diagram of a system for collecting organic carbon content data of a solid sample according to an embodiment of the present invention;
in fig. 2: 1. a function shutdown module; 2. a slope change monitoring module; 3. a detection time setting module; 4. and a data acquisition ending judgment module.
Fig. 3 is a flowchart of an implementation of the method for acquiring organic carbon content data of a solid sample according to an embodiment of the present invention.
Fig. 4 is a schematic diagram of the peak shape of carbon dioxide in air generated during sample replacement according to an embodiment of the present invention.
Fig. 5 is a schematic diagram of a peak shape (taking C210420015 as an example) of data collection in measurement of a raw sample provided by an embodiment of the present invention.
FIG. 6 is a schematic diagram of the peak shape (taking C210420015 as an example) of the data collected by the sample measurement after the application of the present invention provided by the embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Aiming at the problems in the prior art, the invention provides a method, a system, equipment and an application for collecting organic carbon content data of a solid sample, and the invention is described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the method for collecting organic carbon content data of a solid sample provided by the invention comprises the following steps:
s101: the automatic acquisition termination function of the electric signals of the closed instrument (Shimadzu TOC-L + SSM 5000);
s102: retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value, and monitoring the slope change in real time;
s103: the curve returns to the baseline, and a dialog box is popped up when a preset slope threshold value is reached, namely whether the analysis is finished or not or the analysis is continued according to the detection setting time;
s104: the operator judges that the data acquisition is finished, and selects to finish the analysis, and then the next sample is detected; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested.
The method for collecting organic carbon content data of a solid sample provided by the present invention can be implemented by other steps, and the method for collecting organic carbon content data of a solid sample provided by the present invention shown in fig. 1 is only one specific example.
As shown in fig. 2, the system for collecting organic carbon content data of a solid sample provided by the invention comprises:
the function closing module 1 is used for closing the automatic acquisition and termination function of the electric signals;
the slope change monitoring module 2 is used for keeping the slope detection function of the peak-shaped curve, setting a lower slope threshold value and monitoring the slope change in real time;
the detection time setting module 3 is used for returning the curve to the baseline, and popping up a dialog box when a preset slope threshold value is reached, namely whether the analysis is finished or not or the analysis is continued according to the detection setting time;
the data acquisition ending judging module 4 is used for judging that the data acquisition is finished by an operator, selecting ending analysis and detecting the next sample; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested.
The technical solution of the present invention is further described below with reference to the accompanying drawings.
As shown in fig. 3, the method for acquiring organic carbon content data of a solid sample calculates the instant slope of a visual interface peak-shaped curve and monitors the change of the slope; and (4) turning off the automatic acquisition termination function of the instrument, and performing the selection of whether to terminate data acquisition or continue data acquisition according to the curve regression baseline instead.
In the invention, the visualization of the instrument electric signal, namely the 'peak', is generally based on the 'slope sensitivity' concept, namely, a threshold value is set in advance to judge whether the bulge of the signal curve can become the peak or not. The signal curve has fluctuation in the measuring process, so that the slope of the curve changes, if the slope of the curve is greater than the set slope sensitivity, the curve is the starting point of the peak, and when the slope of the curve is reduced below the slope sensitivity, the curve is the end point of the peak, and the curve between the starting point and the end point is the peak.
The method for judging whether the bulge of the signal curve can become a peak comprises the following steps:
the formula for calculating the starting point of the peak of the curve is:
div (i, j) represents an objective coefficient of the calculated current curve peak i and the set curve peak j, and time (i), time (j) respectively represents data time from the beginning to the change of the current curve peak i and the set curve peak j, a numerator is an absolute value of a time difference between the change of the current curve peak i and the change of the set curve peak j, and a denominator is a sum of the change of the time between the change of the current curve peak i and the change of the set curve peak j;
the end point formula for the peak of the curve is calculated as:
αdiv(i,j)+βyi+λyj；
wherein div (i, j) represents the end point correlation degree of the current curve peak i and the set curve peak of j, yiAnd yjRespectively representing the memory rates of curve peaks i and j; α, β, λ are the weight values of the features.
The slope calculation equation of the curve in the data acquisition process of the instrument (Shimadzu TOC-L + SSM5000) is as follows: assuming that f (X, Y) is 0 and P (X, Y) is any point on the curve, the slope of the point on the curve is calculated. I.e., the derivative of the function f (X, y) at 0 and X. The equation f (x, y) is set to be 0, a function y (y) (x) is determined, the equation is substituted with y (x) to obtain an identity f [ x, y (x) 0, and the full derivative of the function is obtained;
Calculating the slope:
the technical effects of the present invention will be described in detail with reference to experiments.
According to the data acquisition method established by the invention, the carbon dioxide peak in the air does not need to be waited in the process of replacing different samples, each sample can be saved by about 4 minutes, and the working efficiency is greatly improved; for a sample with a complex matrix, the data acquisition is complete and objective, the accuracy of the detection result is greatly improved, and the precision of the repeated measurement of the sample is improved.
Fig. 4 is a schematic diagram of the peak shape of carbon dioxide in air generated during sample replacement according to an embodiment of the present invention.
Fig. 5 is a schematic diagram of a peak shape (taking C210420015 as an example) of data collection in measurement of a raw sample provided by an embodiment of the present invention.
FIG. 6 is a schematic diagram of the peak shape (taking C210420015 as an example) of the data collected by the sample measurement after the application of the present invention provided by the embodiment of the present invention.
TABLE 1 comparison of data from sample measurements before and after the application of the invention
As can be seen from the test data in Table 1, the influence on the measurement results of TC before and after the present invention is small because the TC is measured at 900 ℃ and the combustion is sufficient; for IC, because the reaction between the sample matrix and phosphoric acid is slow, the data acquisition process is terminated early, the original IC data acquisition is incomplete, the final data is small, and the TOC value is large.
After the method is utilized, the data acquisition is complete, the IC content can be objectively reflected, and the data accuracy is high. Taking the standard sample GSS-8 as an example, the reference TOC value is 0.30%, the original calculation result is 0.694%, and the current result is 0.303%, which is relatively accurate.
It should be noted that the embodiments of the present invention can be realized by hardware, software, or a combination of software and hardware. The hardware portion may be implemented using dedicated logic; the software portions may be stored in a memory and executed by a suitable instruction execution system, such as a microprocessor or specially designed hardware. Those skilled in the art will appreciate that the apparatus and methods described above may be implemented using computer executable instructions and/or embodied in processor control code, such code being provided on a carrier medium such as a disk, CD-or DVD-ROM, programmable memory such as read only memory (firmware), or a data carrier such as an optical or electronic signal carrier, for example. The apparatus and its modules of the present invention may be implemented by hardware circuits such as very large scale integrated circuits or gate arrays, semiconductors such as logic chips, transistors, or programmable hardware devices such as field programmable gate arrays, programmable logic devices, etc., or by software executed by various types of processors, or by a combination of hardware circuits and software, e.g., firmware.
The above description is only for the purpose of illustrating the present invention and the appended claims are not to be construed as limiting the scope of the invention, which is intended to cover all modifications, equivalents and improvements that are within the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A method for collecting organic carbon content data of a solid sample is characterized by comprising the following steps:
calculating the instant slope of the visual interface peak-shaped curve and monitoring the change of the slope;
closing the automatic acquisition termination function of the instrument, recording the data of curve change and monitoring the slope;
and judging whether to terminate data acquisition or continue data acquisition according to the curve regression baseline.
2. The method of collecting organic carbon content data of a solid sample according to claim 1, wherein the method of collecting organic carbon content data of a solid sample comprises the steps of:
firstly, closing the automatic acquisition termination function of an electric signal of an instrument;
secondly, retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value, and monitoring the slope change in real time;
thirdly, the curve returns to the baseline, a dialog box pops up when the curve reaches a preset slope threshold, and whether the analysis is finished or the analysis is continued according to the detection setting time;
fourthly, judging that the data acquisition is finished, selecting to finish the analysis, and detecting the next sample; judging that the data acquisition is not finished, selecting to continue analyzing, and continuously acquiring data by the instrument according to the time set by detection until the data acquisition is finished; the next sample is tested.
3. The method for collecting organic carbon content data of a solid sample according to claim 2, wherein the method for collecting organic carbon content data of a solid sample sets a threshold value to determine whether a protrusion of a signal curve can become a peak; in the process, a signal curve has fluctuation, so that the slope change of the curve is brought, and if the slope of the curve is greater than the set slope sensitivity, the curve is the starting point of a peak; when the slope of the curve falls below the slope sensitivity, it is the end point of the peak, and the peak is located between the start point and the end point.
4. The method for collecting organic carbon content data of a solid sample according to claim 3, wherein the step of determining whether the protrusion of the signal curve can be peaked comprises:
the formula for calculating the starting point of the peak of the curve is:
div (i, j) represents an objective coefficient of the calculated current curve peak i and the set curve peak j, and time (i), time (j) respectively represents data time from the beginning to the change of the current curve peak i and the set curve peak j, a numerator is an absolute value of a time difference between the change of the current curve peak i and the change of the set curve peak j, and a denominator is a sum of the change of the time between the change of the current curve peak i and the change of the set curve peak j;
the end point formula for the peak of the curve is calculated as:
αdiv(i,j)+βyi+λyj；
wherein div (i, j) represents the end point correlation degree of the current curve peak i and the set curve peak of j, yiAnd yjRespectively representing the memory rates of curve peaks i and j; α, β, λ are the weight values of the features.
5. The method for collecting organic carbon content data of a solid sample according to claim 2, wherein the slope calculation equation of the data collection process curve of the method for collecting organic carbon content data of a solid sample is as follows: the measuring result signal forms a curve equation with f (X, Y) being 0, P (X, Y) being any point on the curve, calculating the slope of the point on the curve, and calculating the derivative of the function f (X, Y) being 0 at X being X;
determining a function y (y) (x) by equation f (x, y) being 0, substituting y (x) into the equation to obtain an identity f [ x, y (x) 0, and calculating the full derivative of the function;
Calculating the slope:
6. a computer device, characterized in that the computer device comprises a memory and a processor, the memory stores a computer program, and the computer program when executed by the processor causes the processor to execute the steps of the method for collecting organic carbon content data of a solid sample according to any one of claims 1 to 5.
7. A computer-readable storage medium storing a computer program which, when executed by a processor, causes the processor to perform the steps of the method for collecting organic carbon content data of a solid sample according to any one of claims 1 to 5.
8. An information data processing terminal, characterized in that the information data processing terminal is used for realizing the steps of the method for collecting the organic carbon content data of the solid sample according to any one of claims 1 to 5.
9. A solid sample organic carbon content data acquisition system for implementing the solid sample organic carbon content data acquisition method according to any one of claims 1 to 5, characterized in that the solid sample organic carbon content data acquisition system comprises:
the function closing module is used for closing the automatic acquisition termination function of the electric signal;
the slope change monitoring module is used for retaining the slope detection function of the peak-shaped curve, setting a lower slope threshold value and monitoring the slope change in real time;
the detection time setting module is used for returning the curve to the baseline, popping up a dialog box when a preset slope threshold value is reached, and judging whether to finish analysis or continue the analysis according to the detection setting time;
the data acquisition ending judging module is used for judging that the data acquisition is finished by an operator, selecting to end the analysis and detecting the next sample; the operator judges that the data acquisition is not finished, selects to continue analyzing, and the instrument continues to separately acquire data according to the time set by detection until the data acquisition is finished; the next sample is tested.
10. The application of the method for collecting the organic carbon content data of the solid sample according to any one of claims 1 to 5 in the processing of the organic carbon content data of the soil sample and the processing of the organic carbon content data of the sediment sample.
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